Manufacturing methods for the production of carbon materials

• US 8,580,870 B2
• Filed: 09/21/2012
• Issued: 11/12/2013
• Est. Priority Date: 04/08/2009
• Status: Expired due to Fees

• Current Assignee: BASF SE
• Original Assignee: EnerG2 Technologies, Incorporated
• Inventors: Costantino, Henry R., Feaver, Aaron, Scott, William D.
• Primary Examiner(s): Cain, Edward
• Application Number:
  US13/624,689
• Publication Number:
  US 20130078443A1
• Time in Patent Office: 417 Days
• Field of Search: 523/309
• US Class Current: 523/309
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01B 3/0021 Carbon, e.g. active carbon, carbon nanotubes, fullerenes; Treatment thereof
• CPC Class Codes: C01B 32/336 characterised by gaseous activating agents
• CPC Class Codes: C08G 8/22 Resorcinol
• CPC Class Codes: C08G 8/28 Chemically modified polycondensates
• CPC Class Codes: C08J 3/12 Powdering or granulating
• CPC Class Codes: C08K 5/04 Oxygen-containing compounds C08K5/0091 takes precedence
• CPC Class Codes: H01G 11/34 characterised by carbonisation or activation of carbon
• CPC Class Codes: H01M 4/96 Carbon-based electrodes
• CPC Class Codes: H01M 8/0234 Carbonaceous material
• CPC Class Codes: Y02E 60/13 Energy storage using capacitors
• CPC Class Codes: Y02E 60/32 Hydrogen storage
• CPC Class Codes: Y02E 60/50 Fuel cells
• CPC Class Codes: Y02P 70/50 Manufacturing or production processes characterised by the final manufactured product
• CPC Class Codes: Y10T 428/2982 Particulate matter [e.g., sphere, flake, etc.]

Abstract

The present application is generally directed to activated carbon materials and methods for making the same. The disclosed methods comprise rapidly freezing synthetically prepared polymer gel particles. The methods further comprise drying, pyrolyzing, and activating steps to obtain an activated carbon material of high porosity. The disclosed methods represent viable manufacturing processes for the preparation of activated carbon materials.

Claims

1. A method for preparing a polymer cryogel, the method comprising:

A) admixing polymer precursors and a catalyst in a solvent to obtain a mixture;

B) allowing the mixture to polymerize to form a gel; and

C) freeze drying the gel to obtain a polymer cryogel,

wherein the solvent is not exchanged for an organic extraction solvent prior to freeze drying.

2. The method of claim 1, wherein the polymer cryogel comprises less than about 1000 ppm of the organic extraction solvent.

3. The method of claim 1, wherein the polymer cryogel comprises a tap density of between about 0.10 g/cc and about 0.60 g/cc.

4. The method of claim 1, wherein freeze drying comprises rapidly freezing the gel in a liquid having a temperature below about −

10°

C.

5. The method of claim 4, wherein the liquid is liquid nitrogen or ethanol.

6. The method of claim 2, wherein the organic extraction solvent is t-butanol or acetone.

7. The method of claim 1, further comprising irradiating the mixture with microwave irradiation.

8. The method of claim 1, wherein the mixture is a suspension.

9. The method of claim 1, wherein the solvent is an aqueous solvent.

10. The method of claim 1, wherein the solvent is an organic solvent.

11. The method of claim 1, wherein the mixture comprises an aqueous phase and an organic phase.

12. The method of claim 1, wherein the mixture is an emulsion.

13. The method of claim 12, wherein the emulsion is selected from a water-in-oil (w/o) emulsion, oil-in-water (o/w) emulsion, oil-in-water-oil (o/w/o) emulsion, water-in-oil-in-water (w/o/w) emulsion, and water-in-oil-in-oil (w/o/o) emulsion.

14. The method of claim 1, wherein the method is for preparing a pyrolyzed polymer cryogel, and the method further comprises pyrolyzing the polymer cryogel.

15. The method of claim 1, wherein the method is for preparing an activated polymer cryogel, and the method further comprises pyrolyzing and activating the polymer cryogel.

16. The method of claim 1, wherein the mixture comprises a surfactant.

17. A method for preparing a polymer cryogel, the method comprising:

A) admixing polymer precursors in a multiphasic system to form polymer gel particles within the multiphasic system; and

B) freeze drying the polymer gel particles to obtain a polymer cryogel.

18. The method of claim 17, wherein the multiphasic system comprises an organic phase and an aqueous phase.

19. The method of claim 17, wherein the multiphasic system comprises a suspension.

20. The method of claim 17, wherein the multiphasic system comprises an emulsion.

21. The method of claim 20, wherein the emulsion is selected from a water-in-oil (w/o) emulsion, oil-in-water (o/w) emulsion, oil-in-water-oil (o/w/o) emulsion, water-in-oil-in-water (w/o/w) emulsion, and water-in-oil-in-oil (w/o/o) emulsion.

22. The method of claim 17, wherein the method is for preparing a pyrolyzed polymer cryogel, and the method further comprises pyrolyzing the polymer cryogel.

23. The method of claim 17, wherein the method is for preparing an activated polymer cryogel, and the method further comprises pyrolyzing and activating the polymer cryogel.

24. The method of claim 17, wherein the multiphasic system comprises a surfactant.

25. The method of claim 17, wherein the polymer gel particles comprise an average particle size of less than about 30 mm.

26. The method of claim 17, wherein the average particle size ranges from about 0.5 mm to about 10 mm.